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Preparation method for high purity catalpic acid and series products like ester and salt thereof

A technology of catalin ester and series products, applied in the field of applied chemistry, can solve the problem of high price and cost, and achieve the effects of low cost, high purity and high edible safety

Inactive Publication Date: 2015-11-25
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, not only consumers have concerns about the safety of industrially prepared CLA, but also there are many problems in the industrialization of CLA itself, such as: the cost of industrialized production of CLA is relatively high; industrially prepared CLA has multiple isomer forms, and Not every isomer has beneficial functions to the human body, among which cis9, trans11-CLA are active isomers with higher safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Preparation of Catalpaic Acid

[0022] The catalpa seeds were collected, dried in an oven at 40°C, and crushed to obtain 1000g of dry powder. After refluxing with 5 times the volume of petroleum ether at less than 60°C for 6 hours, a green triglyceride crude extract was obtained. The oil yield was 28.2%. . Take 50mL of the crude triglyceride extract and add 200mL of 2M90% potassium hydroxide ethanol solution and saponify for 2h at 60℃ under nitrogen protection, add 50mL of water and then add 50mL petroleum ether three times to extract the non-saponifiable compounds, then add 6M hydrochloric acid 100mL After neutralization and acidification, the upper layer is extracted with petroleum ether to obtain a petroleum ether solution, and then after vacuum rotary evaporation, a crude catalpaic acid extract is obtained. The crude catalpaic acid was dissolved in ethanol and crystallized at 4°C under normal pressure for 8 hours to remove saturated fatty acids. The obtain...

Embodiment 2

[0024] Example 2: Preparation of Catalpaic Acid

[0025] The catalpa tree seeds are collected, dried in sunlight and pulverized to obtain 1000g of dry powder with a particle size of 0.4-0.5mm, and extracted with supercritical CO2 under the conditions of 30MPa and 40°C (HA221-50- produced by Huaan Supercritical Extraction Plant in Nantong City, Jiangsu) 06 type supercritical extraction device) 2h, the green triglyceride crude extract (crude oil) is obtained under the separation pressure of 15MPa and the separation temperature of 50℃, the oil yield is 30.2%; the crude oil is degummed, deacidified, decolorized, After deodorization and dewaxing, it is refined to obtain triglycerides. Take 50mL of the crude triglyceride extract and add 200mL of 2M90% potassium hydroxide ethanol solution and saponify for 2h at 60℃ under nitrogen protection, add 50mL of water and then add 50mL petroleum ether three times to extract the non-saponifiable compounds, then add 6M hydrochloric acid 100mL Aft...

Embodiment 3

[0027] Example 3: Preparation of catalpa sodium

[0028] The catalpa seeds are collected, dried in an oven at 40°C and crushed to obtain 1000g of dry powder. After leaching with 5 times the volume of a mixed solution of chloroform and methanol (volume ratio of 1:1) at room temperature for 24 hours, green catallic acid triglycerides are obtained. The crude ester extract has an oil yield of 29.7%. Take 100mL of crude triglyceride extract and add 400mL of 2M90% sodium hydroxide ethanol solution and saponify for 2h at 60℃ under nitrogen protection, add 1000mL of water and then add 100mL petroleum ether for three times to extract the non-saponifiable compounds, then add 200mL of 6M hydrochloric acid After neutralization and acidification, the upper layer was extracted with petroleum ether to obtain a petroleum ether solution. The crude catalpaic acid was crystallized at 4°C under normal pressure for 10 hours to remove saturated fatty acids, and then under normal pressure at minus 40°C...

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Abstract

The invention relates to a preparation method for high purity catalpic acid and series products like ester and salt thereof. According to the invention, catalpa seed is used as a raw material, and catalpic triglyceride is extracted; catalpic triglyceride undergoes saponification and acidification so as to obtain catalpic acid; catalpic acid is esterified so as to obtain catalpic acid ester, or catalpic acid ester is prepared by directly esterifying catalpic triglyceride; obtained catalpic acid and catalpic acid ester are subjected to separation through two-step freezing crystallization so as to obtain catalpic acid and catalpic acid ester with purity of 95 to 98%; and n catalpic acid and catalpic acid ester with purity of 95 to 98% undergo saponification so as to obtain catalpic acid salt with purity of 95 to 98%. Compared with the prior art, the method provided by the invention has the advantages of simple process, low cost, high purity of obtained catalpic acid and ester and salt thereof and wide application prospects.

Description

Technical field [0001] The invention relates to the technical field of applied chemistry, in particular to a method for preparing high-purity catalpic acid and its esters and salts and other series products, and specifically relates to the extraction and preparation of high-purity catalpicacid from Catalpaovata seeds And its ester and salt methods. Background technique [0002] Conjugated fatty acids are fatty acids containing more than two conjugated double bond systems. The most common conjugated fatty acids are stearidienic acid and stearidienic acid, namely conjugated linoleic acid (CLA) and co- Conjugated linolenic acid (CLNA), where CLA is the conjugated form of linoleic acid and CLNA is the conjugated form of α-linolenic acid. CLA and CLNA have different isomers due to the position and configuration of the double bond, 9cis, 11trans-conjugated linoleic acid (cis9, tras11-18:2), 10trans, 12cis-conjugated Oleic acid (tras10, cis12-18:2) and punicic acid (cis9, tras11, cis1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/12C07C27/02C07C51/43C07C69/587C07C67/03C07C67/08C07C67/52C07C51/41A61K31/202A61K31/232A61P9/10A61P3/06A61P5/50
CPCY02P20/54
Inventor 袁高峰孙海燕陈小娥
Owner ZHEJIANG OCEAN UNIV
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